CHEM 2241

Analytical Chemistry I
Lecture + Lab (6 Credits)
Dr. Edmund C. M. TSE
Week 1
[email protected]
 What is Analytical Chemistry?

Class Activity

Think – Pair – Share

1. Think by yourself
2. Pair up to discuss with your neighbor
3. Share with the rest of the class
 Analytical Chemistry

• Separate, Identify, Measure

• Instruments

• Qualitative Methods • Calibration Curves

• Quantitative Practices • Statistics

• Unknowns • Sample Preparation

• Reference Materials • Isolate Analytes
• Standards
Student Population

• 1st Year
• 2nd Year
• 3rd Year
• 4th Year

• Exchange Students
• Non-local Students

• Chemistry Majors
• Other Majors
What do you want to learn from CHEM2241?

Class Activity

Think – Pair – Share

1. Think by yourself
2. Pair up to discuss with your neighbor
3. Share with the rest of the class
 General Learning Goals
Useful
This Class (core level-2 & 1st A Chem course)
Future Classes in Your Major
Other Classes
Graduate School
Future Career
Life

Follow-up: CHEM3241 A Chem II: Chemical Instrumentation (Core)

Advanced: CHEM4241 Modern Instrumentation and Applications
CHEM4242 Analytical Chemistry
Elective: CHEM3242 Food and Water Analysis
 Course Learning Goals
Theoretical Knowledge
Basic Principles: Chemical Analysis
Chemical Equilibrium
Stoichiometric Reactions

Practical Skills
Measurements: Error Analysis
Quality Assurance
Equipment Calibration
Data Acquisition
Data Processing
 Course Content
Method:
Analog and Digital Measurements
Accuracy and Precision
Signal Amplification

Statistics:
Comparing Means and Deviations
Calibration Curves (Limit of Detection)
Least Square Fit for Linear Plots

Quality Assurance:
Validation of Procedures
 Course Topics

Instruments
Calibration
Measurement

Chemical Equilibrium
Acid-base Reactivity
Complexation Reactivity
Precipitation Reactivity

Statistical Analysis
Central Limit Theorem, T-test, P-value
 Online Syllabus and Regulations
https://webapp.science.hku.hk/sr4/servlet/enquiry?Type=Course&course_c
ode=CHEM2241
Course Descriptors: A, B, C, D, Fail
https://www.chemistry.hku.hk/download/programme/CHEM2241_2019.pdf

What it takes to get an A?

Demonstrate thorough grasp of the subject.
Show evidence of strong analytical abilities, logical and
independent thinking, and ability to apply knowledge to a wide
range of complex, familiar and unfamiliar situations.
Demonstrate highly proficient lab skills and techniques and critical
use of data and results to draw appropriate and insightful
conclusions.
Demonstrate highly effective organization and presentation skills
“Theoretical & Practical”
“You are Responsible for Your Own Success”

Activities No. of Hours

Laboratory 24
Lectures 24
Tutorials 6
Reading / Self Study 100

Textbook
Skoog, West, Holler and Crouch
"Fundamentals of Analytical Chemistry“
Cengage Learning
Relevant Book Chapters
Lab Notebook
Lab Notebook
More info on
how to keep a
tidy lab
notebook for
easy lookup will
be posted on
Moodle
Lab Notebook & Data Sheet
 Pre-lab
Read lab manual carefully beforehand, prepare pre-lab document

EXPT 1 Calibration of a 25-mL pipette

EXPT 2 Determination of iron content in minerals

by redox titration

EXPT 3 Determination of iron content in food

by spectrophotometry

EXPT 4 Determination of nickel using dimethylglyoxime

EXPT 5 Measurement and data acquisition

 Analytical Chemistry – What is it?
 Analytical Chemistry Definitions
 “Analytical chemistry involves separating, identifying and determining
the relative amounts of the components in a sample of matter”
• Fundamentals of Analytical Chemistry, Skoog, West & Holler, pg. 1

 “Analytical chemistry is concerned with the theory and practice of

methods used to determine the composition of matter”
• Quantitative Analysis, Day & Underwood, pg. 1

 “Analytical chemistry is the field of chemistry dealing with the theory,

development and practice of methods used to probe the composition
of all phases of matter”

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The Goals of Chemical Analysis
1. To identify what is present in a sample
(Qualitative analysis)

2. To determine how much (the amount of)

analyte is present in a sample (Quantitative
analysis)

 Analyte: Molecule that we are determining

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General steps in chemical analysis
 Formulating the question - “What information is
needed?”
 Selecting analytical procedures
 Acquiring the sample (Sampling)
 Processing the sample
 Eliminating interferences
 Calibrating and Measuring Concentration
 Calculating Results
 Evaluating Results by estimating reliability
 Reporting and interpretation
 Drawing conclusion(s)
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 A case study of chemical analysis

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The Total Diet Study (TDS) takes several years in
preparation and execution
 Food consumption survey (FCS) in 2005 – 2007
– >1400 food items identified
 1st HKTDS in 2010 – 2011
– 150 food items
– 3 samples of each item
– 1800 samples
– 600 composite samples
 Laboratory analysis
– Food Research Laboratory of Center for Food Safety (CFS) and
Government Laboratory
– Analysis of 130 substances (contaminants and nutrients)
– Metal contents (Al, Sb, Cd, Pb, Ni, Sn, V) determined by high resolution
inductively coupled plasma-mass spectrometry (ICP-MS) and gas
chromatography-ICP-MS (for methylmercury)

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Standard methods of analysis

eurachem.org Eurachem is a network of organizations in Europe having the objective

of establishing a system for the international traceability of chemical
measurements and the promotion of good quality practices.

www.nist.gov
9/3/2018
National Institute of Standards
CHEM2241
and Technology, USA 19
“Standard method of analysis of foods for As,
Cd, Cr, Hg and Pb by ICP-MS” of the US FDA
 Sample preparation by microwave digestion
 Instrument setup
– Tuning of the instrument
– Internal standards
– Integration time
 Determination of the metals
– Pre-analysis scan for the presence of internal standard elements and high
levels of analyte elements
– Analysis in quantitation mode
– Use Fortified Analytical Solution (FAS) to check recovery
 Analytical quality control
– Check for interference and instrument drift
– Linearity of calibration curve
– Determination of Limit of Quantification (LOQ) and Detection Limit (LOD)
– Check the True Value Recovery of certified values of Standard Reference
Materials (SRM)
http://www.fda.gov/downloads/Food/FoodSafety/FoodContaminantsAdulteration/Metals/UCM272693.pdf

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 http://www.who.int/foodsafety/publications/chem/en/lowlevel_may1995.pdf

Limit of detection (LOD)

Non-quantifiable (NQ)

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Steps in
Quantitative
Analysis Standard solution,
Internal standard,
Pipet calibration

Incineration,
Microwave digestion

Volumetric methods,
Gravimetric methods,
Spectroscopy
Average,
Significant figures,
Error analysis

Statistical tests
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Topics not covered in lectures in details but are
important in learning of analytical chemistry
 Chapter 1 The nature of analytical chemistry
 Feature 1-1 Deer Kill
 Chapter 2 Chemicals, apparatus, and unit operations
of analytical chemistry
 Grade of chemicals, balance operation, weighing by
difference, filtration and ignition of precipitates
 (Volumetric apparatus – types, classes and tolerances,
calibration will be discussed)
 Chapter 3 Using spreadsheets in analytical chemistry
 Chapter 4 Calculations used in analytical chemistry
 Concentration: molar, parts per million and parts per
billion (ppm and ppb)

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Tools and Apparatus in the Laboratory
Chapter 2D, 2H, and 2I

 Laboratory notebook
 Analytical balance
 Glassware
 Pipet
 Buret
 Volumetric flask

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Analytical Balance
Analytical data are based on mass rather than weight - so that the
results will not depend on location.

Analytical balance Microbalance

Good-quality balances calibrate themselves with internal weights to correct

for variations in the force of gravity, which can be as great as 0.3%, from place
to place.
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 Analytical Balance
 Capable of weighing masses accurately with uncertainties
down to  0.0001 g, i.e.,  0.1 mg. (Some models down to 0.01
mg).

 Weighing procedure
 Use a brush to clean the balance pan before every weighing
 Use finger cots or Kimwipe to pick up objects being
weighed. Never use fingers directly on the object.
(Fingerprint residue can add significant error)
 Keep doors closed when weighing
 Allow signal to stabilize for a consistent amount of time
before recording mass
 Never weigh material directly on the pan – use a container
 If signal “drifts”, this could indicate a static electricity
problem – wipe anti-static solution on balance
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Analytical Balance - Principle of Operation

The position sensor detects displacement of the lever arm;

the servo amplifier sends a current through the force
compensation wire coil in the field of the permanent
Schematic diagram of electronic balance magnet. The current is converted into mass, which is
C. Berg, “The Fundamentals of Weighing Technology” (1996) displayed

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Tolerances of Laboratory Apparatus
Apparatus Capacity Error* relative error
(volume, weight)
volumetric flask 100 mL 0.15 mL 1.510-3
pipet 25 mL 0.06 mL 2.410-3
micropipet 1 - 1000 μL -- 110-2
buret 50 mL 0.05 mL 110-3
analytical balance 200 g 0.1 mg

*Class B volumetric apparatus. Tolerances for Class A  half of Class B.

Typical sample weight = 1 g

Relative error of a balance = 0.1×10-3/1 = 1×10-4
The most accurate apparatus in the laboratory is the analytical balance.
Therefore, laboratory apparatus are calibrated using the analytical balance.
Reference:
Vogel’s Textbook of Quantitative Chemical analysis, 5/e, p. 78-89, Longman (1989).
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 Units
Predominantly SI units these days

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